CN101885622B - Preparation method of SiC coated mullite complex coating of C/C composite material - Google Patents
Preparation method of SiC coated mullite complex coating of C/C composite material Download PDFInfo
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- CN101885622B CN101885622B CN2010101983666A CN201010198366A CN101885622B CN 101885622 B CN101885622 B CN 101885622B CN 2010101983666 A CN2010101983666 A CN 2010101983666A CN 201010198366 A CN201010198366 A CN 201010198366A CN 101885622 B CN101885622 B CN 101885622B
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Abstract
The invention discloses a preparation method of a SiC coated mullite complex coating of a C/C composite material, which comprises the following steps: evenly mixing tetraethoxysilane, absolute ethyl alcohol and distilled water to obtain a tetraethoxysilane solution; mixing Al(NO3)3 aqueous solution with the tetraethoxysilane solution to obtain sol; dispersing nano SiC powder into the sol to obtain a suspension sol; aging and drying the suspension sol into dried gel, grinding the dried gel in an agate mortar, and then putting the ground dried gel into a crucible and sintering to obtain SiC coated mullite powder; dissolving the coated mullite powder into isopropanol to prepare into suspension and then adding iodine simple substance, clipping C/C composite material samples with a SiC inner coating on the cathode clip in a hydrothermal kettle; putting the hydrothermal kettle in an oven for hydrothermal electrophoresis reaction and then naturally cooling to room temperature; and taking out the samples and drying to obtain the SiC coated mullite complex coating of the C/C composite material. The prepared SiC coated mullite complex coating of the C/C composite material has excellent bond, even thickness, compact surface and excellent physical and chemical compatibility.
Description
Technical field
The present invention relates to a kind of preparation method of C/C matrix material compound coating, be specifically related to the surperficial even compact of a kind of preparation, and uniform in thickness does not have the preparation method of the C/C matrix material SiC coated mullite compound coating of penetrating crack and pin hole generation.
Background technology
Carbon/carbon compound material (C/C) is to be the C-base composte material of wild phase with the thomel; Have characteristics such as light specific gravity, high-strength and high-modulus property, high thermal stability, high heat-conductivity conducting ability, low density, low thermal coefficient of expansion, anti-ablation, corrosion-resistant, stable friction factor; The characteristic that particularly goes up not down with temperature rising mechanical property is the high-temperature material of ideal aerospace and other industrial circle.Yet; Its many above-mentioned character only could keep under inert atmosphere; Research shows that the C/C matrix material is beginning to take place oxidizing reaction above under 370 ℃ the oxidizing atmosphere, and speed of response also can increase rapidly in the time of 500 ℃; Oxidation weight loss will make the mechanical property of C/C matrix material obviously descend, thereby limit it as high temperature protection or the widespread use of anti-ablator under oxidizing atmosphere.Therefore, the anti-oxidation C/C matrix material key in application that becomes.
At present; The coating for preparing high temperature oxidation resisting at the C/C composite material surface; Be ORC, be considered to solve the effective ways of carbon/carbon compound material high temperature oxidation protection question, its essence is to utilize high temperature coating isolation from oxygen and C/C matrix to reach anti-oxidation purpose.But single coating is difficult to effectively protect carbon/carbon compound material to avoid oxidation for a long time.At present, coating system is to compound coating system development, mainly with the SiC stupalith that has the good physical chemical compatibility with the C/C matrix as buffer coating, have the top coating of good thermal stability, consistency and resistance oxygen ability then in its surface-coated.
Up to the present, have as the material of top coating a variety of, the coating system of the C/C matrix material of having developed mainly contain glass coating [Zhang Weigang, Cheng Huiming, Shen Zuhong, etc.TiC is to the influence [J] of C-SiC-B4C matrix material oxidation behavior, novel charcoal material, 1998,13 (1): 13-18], metallic coating [Worrell; Wayne L, Lee K N.Hightemperature alloys, United States Patent; 6127047,2000.], ceramic coating [once mediate banyan, Zheng Changqing; The anti-oxidation research [J] of the .C/C of Li He army matrix material MoSi2 coating. matrix material journal, 1997,14 (3): 37-40] and compound coating [Huang J F; Zeng X R, Li H J, et al.Mullite-Al2O3-SiC oxidation protective coating forcarbon/carbon composites [J] .Carbon; 2003,41 (14): 2825-2829.], and compound coating comprises gradient cladding and bilayer and laminated coating etc.
The preparation method of C/C matrix material ORC has a lot, mainly contains entrapping method [Huang J F, Li H J; Zeng XR; Li H J, et al.Influence of the preparing temperature on phase, microstructure and anti-oxidationproperty of SiC coating for C/C composites [J] .Carbon; 2004; 42 (8-9): 1517-1521.], chemical vapor deposition (CVD) [Cheng L F, Xu Y D, Zhang L T; Et al.Preparation of An Oxidation ProtectionCoating for C/C Composites by Low Pressure Chemical Vapor Deposition [J] .Carbon; 2000, (38): 1493-1498.], molten slurry method [Joshi A.Coating with Particulate Ddispersions for HighTemperature Oxidation Protection of Carbon and C/C composites [J] .Composites (Part A), 1997; 28 (2): 181-189], flame plating and plasma spraying method [Cheng Laifei; Zhang Litong. liquid phase method prepares the anti-oxygen of C/C and ends the liquid spreading research [J] of coating. aviation journal, 1996,17 (4): 508-510] etc.These methods or high to equipment requirements, equipment and instrument are relatively more expensive; Preparation technology is relatively harsher, and preparation condition is more extreme; Perhaps complex process, preparation cycle is long, and is repeatable poor.
Summary of the invention
The technical problem that the present invention will solve is: to the shortcoming and the deficiency of prior art existence; The preparation method of the C/C matrix material SiC coated mullite compound coating that a kind of technology is simple, preparation cost is low is provided; Prepared C/C matrix material SiC coated mullite compound coating bonding force is good, thickness even, surface compact, and the good materialization consistency of tool.
For achieving the above object; The technical scheme that the present invention adopts is: 1) get and use the pH value of hydrochloric acid conditioning solution to be 2-4 after 5ml tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water mix, the normal temperature lower magnetic force stirs 30-60min makes tetraethoxy prehydrolysis get teos solution; 2) get the analytically pure Al (NO of 25.12g
3)
39H
2The zero(ppm) water that O is dissolved in 10-20ml magnetic agitation 30-60min is at normal temperatures processed Al (NO
3)
3The aqueous solution; 3) with step 2) preparation Al (NO
3)
3The aqueous solution mixes back normal temperature magnetic agitation 2-4h with the teos solution of step 1) preparation and gets colloidal sol, and the pH value of in this process, using ammoniacal liquor to regulate colloidal sol is 4.5-5.5; 4) get the 5-8g mean particle size be the nano SiC powder of 40nm be scattered in adopt in the described colloidal sol ultra-sonic dispersion make the nano SiC powder in colloidal sol, be uniformly dispersed suspension colloidal sol; 5) with after the suspension colloidal sol ageing 24-48h, placing 60 ℃ of oven dry of baking oven is xerogel, again xerogel in agate mortar, grind broken after; Place alumina crucible, put into retort furnace, it is 5 ℃/min that temperature rise rate is set; Be warming up to 1150 ℃ from room temperature; Insulation 2h cools to room temperature then with the furnace, makes SiC coated mullite powder; 6) getting 3-5gSiC coated mullite powder joins in the Erlenmeyer flask; Again the Virahol of 100-200ml is poured into and processed suspension-s in the Erlenmeyer flask, after in suspension-s, adding the 0.3-0.4g elemental iodine again behind the ultrasonic concussion of suspension-s 30min, the magnetic agitation 12h, carry out ultrasonic concussion 30min, magnetic agitation 12h again; 7) suspension-s of step 6) preparation is poured in the hydrothermal reaction kettle, compactedness is controlled at 65-70%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; Again the positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply; Hydrothermal temperature begins electrophoresis after being controlled at 80-300 ℃ of insulation 1h, and electrophoresis time is controlled at 10-60min, and voltage of supply is controlled at 120-240V; The hydro-thermal electrophoresis is turned off baking oven and is naturally cooled to room temperature by it after finishing; 8) last, open water heating kettle taking-up samples dried and get C/C matrix material SiC coated mullite compound coating.
SiO in the tetraethoxy of the present invention
2Content more than or equal to 28%; The pH=10.7 of ammoniacal liquor; It is the ultrasonic generator of 100-300W that ultra-sonic dispersion adopts power; The drying of step 8) is in 80-100 ℃ of drying in electric drying oven with forced convection.
The present invention adopts sol-gel method at C/C composite material surface coated mullite, to improve the antioxidant property of its particulate.And then prepare SiC coated mullite compound coating with the pulsed hydrothermal electrophoresis sedimentation.The SiC coated mullite uses as the C/C-SiC top coating and has the following advantages: (1) mullite has higher thermostability and antioxidant property, and fusing point can effectively improve the oxidation-resistance of C/C matrix material greater than 1800 ℃.(2) and the undercoat of SiC and C/C matrix material is formed identically, the materialization consistency is fine, and hot matching is fine, can not produce elevated temperature heat stress.The SiC coated mullite compound coating bonding force that the present invention makes is stronger, has good materialization consistency; The compound coating uniform in thickness, surface compact does not have pin hole and penetrating crack to occur; Can be at 1500 ℃ of still airs protection C/C matrix material 150h, oxidation weight loss only 0.8%.
Description of drawings
SiC coated mullite compound coating surface (XRD) collection of illustrative plates of Fig. 1 embodiment of the invention 1 preparation, wherein X-coordinate is diffraction angle 2 θ, unit is °; Ordinate zou is a diffraction peak intensity, and unit is a.u.; ESEM (SEM) photo on the SiC coated mullite compound coating surface of Fig. 2 embodiment of the invention 1 preparation; Section surface sweeping Electronic Speculum (SEM) photo of the SiC-C/C sample of the SiC coated mullite compound coating protection of Fig. 3 embodiment of the invention 1 preparation.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Embodiment 1:1) gets 5ml SiO
2Content mix the back more than or equal to 28% tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water to use the pH value of hydrochloric acid conditioning solution be 4, normal temperature lower magnetic force stirring 1h makes tetraethoxy prehydrolysis get teos solution; 2) get the analytically pure Al (NO of 25.12g
3)
39H
2O is dissolved in the zero(ppm) water of 10ml at normal temperatures, and magnetic agitation 30min processes Al (NO
3)
3The aqueous solution; 3) with step 2) preparation Al (NO
3)
3The aqueous solution mixes back normal temperature magnetic agitation 2-4h with the teos solution of step 1) preparation and gets colloidal sol, and in this process, using the pH value of the ammoniacal liquor adjusting colloidal sol of pH=10.7 is 4.5; 4) get the 5g mean particle size be the nano SiC powder of 40nm be scattered in adopt in the described colloidal sol power be the ultrasonic generator ultra-sonic dispersion of 100-300W make the nano SiC powder in colloidal sol, be uniformly dispersed suspension colloidal sol; 5) with after the suspension colloidal sol ageing 24h, placing 60 ℃ of oven dry of baking oven is xerogel, again xerogel in agate mortar, grind broken after; Place alumina crucible, put into retort furnace, it is 5 ℃/min that temperature rise rate is set; Be warming up to 1150 ℃ from room temperature; Insulation 2h cools to room temperature then with the furnace, makes SiC coated mullite powder; 6) getting 3gSiC coated mullite powder joins in the Erlenmeyer flask; The Virahol of 100ml is poured into again and processed suspension-s in the Erlenmeyer flask, it is that in suspension-s, to add behind the ultrasonic concussion of the ultrasonic generator 30min, magnetic agitation 12h of 100-300W behind the 0.3g elemental iodine be the ultrasonic concussion of ultrasonic generator 30min, the magnetic agitation 12h of 100-300W again at power again that suspension-s is adopted power; 7) suspension-s of step 6) preparation is poured in the hydrothermal reaction kettle, compactedness is controlled at 70%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; Again the positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply; Hydrothermal temperature begins electrophoresis after being controlled at 80 ℃ of insulation 1h, and electrophoresis time is controlled at 60min, and voltage of supply is controlled at 120V; The hydro-thermal electrophoresis is turned off baking oven and is naturally cooled to room temperature by it after finishing; 8) last, open water heating kettle take out sample in electric drying oven with forced convection in 80 ℃ of dry C/C matrix material SiC coated mullite compound coatings.
Can find out that by Fig. 1 the compound coating surface is mainly mullite crystalline phase and SiC crystalline phase, the successfully preparation of SiC coated mullite compound coating is described.
As can be seen from Figure 2, coatingsurface is made up of many tiny particulate state crystal grain, and particle is tightly packed, and coatingsurface does not have tiny crack to occur, and is dense and even.
As can be seen from Figure 3, adopt the prepared SiC coated mullite compound coating thickness of water heat electrophoresis deposition method greatly about 63.7? About m.Whole coat-thickness is even and fine and close, combines between the inside and outside coating closely, does not have tangible interface layer and penetrance defective and exists, and explains that coatings prepared is better.
Embodiment 2:1) gets 5ml SiO
2Content mix the back more than or equal to 28% tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water to use the pH value of hydrochloric acid conditioning solution be 3, normal temperature lower magnetic force stirring 40min makes tetraethoxy prehydrolysis get teos solution; 2) get the analytically pure Al (NO of 25.12g
3)
39H
2O magnetic agitation at normal temperatures is dissolved in that 30min processes Al (NO in the zero(ppm) water of 15ml
3)
3The aqueous solution; 3) with step 2) preparation Al (NO
3)
3The aqueous solution mixes back normal temperature magnetic agitation 2-4h with the teos solution of step 1) preparation and gets colloidal sol, and in this process, using the pH value of the ammoniacal liquor adjusting colloidal sol of pH=10.7 is 5; 4) get the 6g mean particle size be the nano SiC powder of 40nm be scattered in adopt in the described colloidal sol power be the ultrasonic generator ultra-sonic dispersion of 100-300W make the nano SiC powder in colloidal sol, be uniformly dispersed suspension colloidal sol; 5) with after the suspension colloidal sol ageing 36h, placing 60 ℃ of oven dry of baking oven is xerogel, again xerogel in agate mortar, grind broken after; Place alumina crucible, put into retort furnace, it is 5 ℃/min that temperature rise rate is set; Be warming up to 1150 ℃ from room temperature; Insulation 2h cools to room temperature then with the furnace, makes SiC coated mullite powder; 6) getting 4gSiC coated mullite powder joins in the Erlenmeyer flask; The Virahol of 150ml is poured into again and processed suspension-s in the Erlenmeyer flask, it is that in suspension-s, to add behind the ultrasonic concussion of the ultrasonic generator 30min, magnetic agitation 12h of 100-300W behind the 0.33g elemental iodine be the ultrasonic concussion of ultrasonic generator 30min, the magnetic agitation 12h of 100-300W again at power again that suspension-s is adopted power; 7) suspension-s of step 6) preparation is poured in the hydrothermal reaction kettle, compactedness is controlled at 65%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; Again the positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply; Hydrothermal temperature begins electrophoresis after being controlled at 150 ℃ of insulation 1h, and electrophoresis time is controlled at 40min, and voltage of supply is controlled at 240V; The hydro-thermal electrophoresis is turned off baking oven and is naturally cooled to room temperature by it after finishing; 8) last, open water heating kettle take out sample in electric drying oven with forced convection in 90 ℃ of dry C/C matrix material SiC coated mullite compound coatings.
Embodiment 3:1) gets 5ml SiO
2Content mix the back more than or equal to 28% tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water to use the pH value of hydrochloric acid conditioning solution be 2, normal temperature lower magnetic force stirring 1h makes tetraethoxy prehydrolysis get teos solution; 2) get the analytically pure Al (NO of 25.12g
3)
39H
2O is dissolved in the zero(ppm) water of 20ml at normal temperatures, and magnetic agitation 30min processes Al (NO
3)
3The aqueous solution; 3) with step 2) preparation Al (NO
3)
3The aqueous solution mixes back normal temperature magnetic agitation 2-4h with the teos solution of step 1) preparation and gets colloidal sol, and in this process, using the pH value of the ammoniacal liquor adjusting colloidal sol of pH=10.7 is 4.5; 4) get the 7g mean particle size be the nano SiC powder of 40nm be scattered in adopt in the described colloidal sol power be the ultrasonic generator ultra-sonic dispersion of 100-300W make the nano SiC powder in colloidal sol, be uniformly dispersed suspension colloidal sol; 5) with after the suspension colloidal sol ageing 48h, placing 60 ℃ of oven dry of baking oven is xerogel, again xerogel in agate mortar, grind broken after; Place alumina crucible, put into retort furnace, it is 5 ℃/min that temperature rise rate is set; Be warming up to 1150 ℃ from room temperature; Insulation 2h cools to room temperature then with the furnace, makes SiC coated mullite powder; 6) getting 5gSiC coated mullite powder joins in the Erlenmeyer flask; The Virahol of 200ml is poured into again and processed suspension-s in the Erlenmeyer flask, it is that in suspension-s, to add behind the ultrasonic concussion of the ultrasonic generator 30min, magnetic agitation 12h of 100-300W behind the 0.4g elemental iodine be the ultrasonic concussion of ultrasonic generator 30min, the magnetic agitation 12h of 100-300W again at power again that suspension-s is adopted power; 7) suspension-s of step 6) preparation is poured in the hydrothermal reaction kettle, compactedness is controlled at 68%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; Again the positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply; Hydrothermal temperature begins electrophoresis after being controlled at 220 ℃ of insulation 1h, and electrophoresis time is controlled at 30min, and voltage of supply is controlled at 160V; The hydro-thermal electrophoresis is turned off baking oven and is naturally cooled to room temperature by it after finishing; 8) last, open water heating kettle take out sample in electric drying oven with forced convection in 100 ℃ of dry C/C matrix material SiC coated mullite compound coatings.
Embodiment 4:1) gets 5ml SiO
2Content mix the back more than or equal to 28% tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water to use the pH value of hydrochloric acid conditioning solution be 3, normal temperature lower magnetic force stirring 1h makes tetraethoxy prehydrolysis get teos solution; 2) get the analytically pure Al (NO of 25.12g
3)
39H
2O is dissolved in the zero(ppm) water of 13ml at normal temperatures, and magnetic agitation 30min processes Al (NO
3)
3The aqueous solution; 3) with step 2) preparation Al (NO
3)
3The aqueous solution mixes back normal temperature magnetic agitation 2-4h with the teos solution of step 1) preparation and gets colloidal sol, and in this process, using the pH value of the ammoniacal liquor adjusting colloidal sol of pH=10.7 is 5.5; 4) get the 8g mean particle size be the nano SiC powder of 40nm be scattered in adopt in the described colloidal sol power be the ultrasonic generator ultra-sonic dispersion of 100-300W make the nano SiC powder in colloidal sol, be uniformly dispersed suspension colloidal sol; 5) with after the suspension colloidal sol ageing 42h, placing 60 ℃ of oven dry of baking oven is xerogel, again xerogel in agate mortar, grind broken after; Place alumina crucible, put into retort furnace, it is 5 ℃/min that temperature rise rate is set; Be warming up to 1150 ℃ from room temperature; Insulation 2h cools to room temperature then with the furnace, makes SiC coated mullite powder; 6) getting 4.5gSiC coated mullite powder joins in the Erlenmeyer flask; The Virahol of 180ml is poured into again and processed suspension-s in the Erlenmeyer flask, it is that in suspension-s, to add behind the ultrasonic concussion of the ultrasonic generator 30min, magnetic agitation 12h of 100-300W behind the 0.38g elemental iodine be the ultrasonic concussion of ultrasonic generator 30min, the magnetic agitation 12h of 100-300W again at power again that suspension-s is adopted power; 7) suspension-s of step 6) preparation is poured in the hydrothermal reaction kettle, compactedness is controlled at 66%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; Again the positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply; Hydrothermal temperature begins electrophoresis after being controlled at 300 ℃ of insulation 1h, and electrophoresis time is controlled at 10min, and voltage of supply is controlled at 200V; The hydro-thermal electrophoresis is turned off baking oven and is naturally cooled to room temperature by it after finishing; 8) last, open water heating kettle take out sample in electric drying oven with forced convection in 85 ℃ of dry C/C matrix material SiC coated mullite compound coatings.
The present invention adopts the pulsed hydrothermal electrophoresis sedimentation; The pulsed hydrothermal electrophoresis sedimentation is meant under the specific physical chemical environment of hydro-thermal; Rely on the effect of DC electric field, powder granule is deposited on from suspension-s to have opposite charges and has the phenomenon on the definite shape electrode.It combines electrophoretic deposition and hydrothermal method advantage, and electrophoretic deposition process is carried out under the supercritical state of hydro-thermal.The water heat electrophoresis deposition legal system is equipped with coating and has the following advantages: (1) the hydro-thermal deposition condition down coating of preparation does not need subsequent crystallization heat treatment, avoided to a certain extent in the later stage heat treatment process, possibly causing curl, defective such as grain coarsening; (2) can avoid adopting conventional high-temperature to apply and the phase transformation and the embrittlement that cause, solve in the coating prepn process thermal damage to a certain extent matrix; (3) to have sedimentation rate fast for this method, and the current efficiency advantages of higher is in the coating that can on complex surfaces and porous matrix, obtain even compact under the simple operation situation.
Claims (5)
1. the preparation method of a C/C matrix material SiC coated mullite compound coating is characterized in that:
1) get 5ml tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water and mix the back and uses the pH value of hydrochloric acid conditioning solution to be 2-4, normal temperature lower magnetic force stirring 1h makes tetraethoxy prehydrolysis get teos solution;
2) get the analytically pure Al (NO of 25.12g
3)
39H
2O is dissolved in the zero(ppm) water of 10-20ml at normal temperatures, and magnetic agitation 30min processes Al (NO
3)
3The aqueous solution;
3) with step 2) preparation Al (NO
3)
3The aqueous solution mixes back normal temperature magnetic agitation 2-4h with the teos solution of step 1) preparation and gets colloidal sol, and the pH value of in this process, using ammoniacal liquor to regulate colloidal sol is 4.5-5.5;
4) get the 5-8g mean particle size be the nano SiC powder of 40nm be scattered in adopt in the described colloidal sol ultra-sonic dispersion make the nano SiC powder in colloidal sol, be uniformly dispersed suspension colloidal sol;
5) with after the suspension colloidal sol ageing 24-48h, placing 60 ℃ of oven dry of baking oven is xerogel, again xerogel in agate mortar, grind broken after; Place alumina crucible, put into retort furnace, it is 5 ℃/min that temperature rise rate is set; Be warming up to 1150 ℃ from room temperature; Insulation 2h cools to room temperature then with the furnace, makes SiC coated mullite powder;
6) getting 3-5gSiC coated mullite powder joins in the Erlenmeyer flask; Again the Virahol of 100-200ml is poured into and processed suspension-s in the Erlenmeyer flask, after in suspension-s, adding the 0.3-0.4g elemental iodine again behind the ultrasonic concussion of suspension-s 30min, the magnetic agitation 12h, carry out ultrasonic concussion 30min, magnetic agitation 12h again;
7) suspension-s of step 6) preparation is poured in the hydrothermal reaction kettle, compactedness is controlled at 65-70%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; Again the positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply; Hydrothermal temperature begins electrophoresis after being controlled at 80-300 ℃ of insulation 1h, and electrophoresis time is controlled at 10-60min, and voltage of supply is controlled at 120-240V; The hydro-thermal electrophoresis is turned off baking oven and is naturally cooled to room temperature by it after finishing;
8) last, open water heating kettle taking-up samples dried and get C/C matrix material SiC coated mullite compound coating.
2. the preparation method of C/C matrix material SiC coated mullite compound coating according to claim 1 is characterized in that: SiO in the said tetraethoxy
2Content more than or equal to 28%.
3. the preparation method of C/C matrix material SiC coated mullite compound coating according to claim 1 is characterized in that: the pH=10.7 of said ammoniacal liquor.
4. the preparation method of C/C matrix material SiC coated mullite compound coating according to claim 1 is characterized in that: it is the ultrasonic generator of 100-300W that said ultra-sonic dispersion adopts power.
5. the preparation method of C/C matrix material SiC coated mullite compound coating according to claim 1 is characterized in that: the drying of said step 8) is in 80-100 ℃ of drying in electric drying oven with forced convection.
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| CN102534731B (en) * | 2012-01-21 | 2014-09-24 | 中国科学技术大学 | Method for preparing vanadium dioxide film through electrophoretic deposition |
| CN102746028A (en) * | 2012-05-26 | 2012-10-24 | 苏州宏久航空防热材料科技有限公司 | Oxide-particle-embedded silicon carbide coating and preparation method thereof |
| CN104030716B (en) * | 2014-06-09 | 2015-10-14 | 西北工业大学 | The method of sol-gel method in-situ synthesis of SiC nano wire modifying carbon/carbon composite material precast body |
| CN107442384B (en) * | 2017-06-26 | 2020-11-06 | 重庆正峰电子有限公司 | Preparation method of nano mullite thermal shock resistant ceramic coating |
| CN108276823B (en) * | 2018-01-17 | 2021-02-12 | 天津中材工程研究中心有限公司 | SiC composite material powder applied to infrared radiation energy-saving coating and preparation method thereof |
| CN109942317A (en) * | 2019-04-25 | 2019-06-28 | 西北工业大学 | Surface of carbon/carbon composite mullite crystal whisker-mullite/yttrium aluminosilicate compound anti-oxidation coating and preparation method |
| CN113929495B (en) * | 2021-10-26 | 2022-11-08 | 西安热工研究院有限公司 | Mullite anti-oxidation coating for composite material and preparation method thereof |
| CN113957379B (en) * | 2021-10-26 | 2024-01-23 | 西安热工研究院有限公司 | N-SiC/Al 2 O 3 Nano composite anti-corrosion coating and preparation method thereof |
| CN113929496A (en) * | 2021-10-26 | 2022-01-14 | 西安热工研究院有限公司 | Mullite high-temperature anti-oxidation coating on surface of composite material and preparation method thereof |
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